EP2896502B1 - Verbundfolie und Verfahren zur Herstellung - Google Patents

Verbundfolie und Verfahren zur Herstellung Download PDF

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Publication number
EP2896502B1
EP2896502B1 EP14151504.9A EP14151504A EP2896502B1 EP 2896502 B1 EP2896502 B1 EP 2896502B1 EP 14151504 A EP14151504 A EP 14151504A EP 2896502 B1 EP2896502 B1 EP 2896502B1
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EP
European Patent Office
Prior art keywords
plasma
adhesion promoter
layer
plated
composite sheet
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
EP14151504.9A
Other languages
English (en)
French (fr)
Other versions
EP2896502A1 (de
Inventor
Ingo KLÜPPEL
Michael Strack
Ingo Rogner
Nicolé Scherf
Gabriella Da Ponte
Danny Havermans
Sabine Paulussen
Bert Verheyde
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Vito NV
ThyssenKrupp Steel Europe AG
Original Assignee
Vito NV
ThyssenKrupp Steel Europe AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Vito NV, ThyssenKrupp Steel Europe AG filed Critical Vito NV
Priority to EP14151504.9A priority Critical patent/EP2896502B1/de
Priority to PCT/EP2015/050779 priority patent/WO2015107152A1/en
Priority to CN201580004774.4A priority patent/CN105939852B/zh
Publication of EP2896502A1 publication Critical patent/EP2896502A1/de
Priority to US15/205,159 priority patent/US20160318294A1/en
Application granted granted Critical
Publication of EP2896502B1 publication Critical patent/EP2896502B1/de
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
    • B32B37/16—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with all layers existing as coherent layers before laminating
    • B32B37/20—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with all layers existing as coherent layers before laminating involving the assembly of continuous webs only
    • B32B37/203—One or more of the layers being plastic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/0008—Electrical discharge treatment, e.g. corona, plasma treatment; wave energy or particle radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00—Processes for applying liquids or other fluent materials
    • B05D1/62—Plasma-deposition of organic layers

Definitions

  • the invention relates to a method of manufacturing a composite sheet, in particular a sandwich sheet, wherein the composite sheet comprises at least two outer metal layers and at least one intermediate polymer layer wherein the polymer layer comprises a thermoplastic polymer. Furthermore, the invention relates to a composite sheet as well.
  • Composite sheets in particular sandwich sheets comprising two outer metal layers and an intermediate polymer layer between both outer metal layers are used to ensure properties of normal bulk metal sheets but additionally providing a reduced weight. These composite sheets allow construction of for example a vehicle with less weight. Additionally, composite sheets in particular sandwich sheets provide damping properties for acoustic noise and high rigidity and stiffness. Not only the mechanical properties of the metal layers in use but also the at least one intermediate polymer layer has a great influence onto the rigidity and stiffness properties, too. Another important aspect of such a composite sheet is the adhesion strength between the metal layers and the polymer layer which has a direct influence on the stiffness and as well as on the rigidity of the composite sheet. The adhesion strength can be measured by the T-peel test according DIN 53282.
  • EP 2 589 438 A1 a plasma surface activation method is disclosed which uses a precursor solution injected as an aerosol into a plasma.
  • the coating of the substrate is achieved by moving the substrate into the plasma including the aerosol.
  • the deposition was carried out for nearly 30 s, which seems to be not applicable to the production of composite sheets using for example a continuous manufacturing process.
  • a further method of manufacturing a composite sheet having two outer layers is known from EP-A-1 593 438 .
  • the plasma coating step is preferably provided inline with the laminating step of the composite material, in particular the sandwich material from which composite sheets, in particular sandwich sheets can be made of. It has been surprisingly found that the manufacturing speed allows including a plasma-coating-step of the inner sides of the metal layers of a composite sheet with the manufacturing step of laminating both metal layers together with the intermediate thermoplastic polymer layer.
  • Composite sheets manufactured according to the present invention show an increase in peel test value which is more than 1.5 times higher than the peel test value of conventional adhesion promoter layer if both inner sides of the metal layers are coated with the plasma polymerized adhesion promoter layer.
  • the increase in peel test value is an important feature of a composite sheet, in particular a sandwich sheet for producing complex shaped parts for example vehicle parts.
  • the plasma coating can be carried out in a separate step. As substrate strip or sheet material can be used.
  • the precursor for providing the adhesion promoter layer is in liquid state.
  • An aerosol is created comprising a support gas and at least one precursor liquid which is injected into the plasma or plasma afterglow.
  • a precursor in a gaseous state can be used and directly injected into the plasma or plasma afterglow without the need of a support gas.
  • a preferred process gas or support gas contains N 2 , CO 2 , Ar and/or He. Good results with respect to an increase of the peel test value of the composite sheet were achieved if the aerosol is generated using a precursor liquid comprising organic acid, in particular organic carboxylic acid, in particular an acrylic acid or methacrylic acid. Other organic acids can also be used.
  • the process gas further comprises at least hydrogen as reactive gas.
  • the combination of for example nitrogen and hydrogen as reactive gas leads to a further increase of the peel test value of manufactured composite sheets.
  • the process gas comprises in maximum 5 vol.-% hydrogen, more preferably in maximum 4 vol.-%, more preferably in maximum 3 vol.-% in order to ensure an increase of peel test value. Yet, it is believed that a minimum amount of 0.1 vol.-% of hydrogen is a lower limit to provide the effect of an increase in peel test value.
  • a plasma polymerized adhesion promoter layer with a thickness of 2 to 50 nm is deposited on the inner side of at least one metal layer. Despite of the low thickness of the adhesion promoter layer a significant increase in adhesion strength can be achieved.
  • the plasma is generated at atmospheric pressure preferably between a first electrode and a second electrode whereby the plasma coating apparatus is equipped in a simple manner.
  • the metal substrates are uncoated steel substrates or steel substrates, which are plated with zinc, zinc-magnesium, chromium-plated or plated on an aluminum-basis.
  • the coatings however additionally provide a protection against corrosion of the steel substrates for example.
  • Other metal substrates are stainless steel, aluminum and its alloys and magnesium and its alloys, zinc, copper or titanium or their combinations or plated metal substrates of the afore mentioned metals.
  • a composite sheet in particular a sandwich sheet, consisting of at least two outer metal layers and at least one intermediate thermoplastic polymer layer, wherein at least one inner side of one outer metal layer comprises a plasma polymerized adhesion promoter layer coated by the inventive method
  • the inventive composite sheet with the increased peel test value enables higher deformation degrees and better T-bend results at small outside radii to produce complex shaped parts without delamination.
  • composite sheet is further improved in that both inner sides of both outer metal layers are coated with an adhesion promoter layer by plasma coating.
  • the plasma polymerized adhesion promoter layer has preferably a thickness of 2 to 50 nm, which allows achieving a reliable increase in peel test value.
  • the outer metal layers are made of an uncoated steel or a steel substrate, which is plated with zinc, zinc-magnesium, chromium-plated or plated on an aluminum-basis in order to provide a high corrosion resistance.
  • Further metals like stainless steel, aluminum and its alloys and magnesium and its alloys, zinc, copper, titanium or their combinations can be used.
  • Fig. 1 shows a schematic view of an embodiment of the manufacturing method according to the present invention.
  • the first and the second metal strip 1, 2 are provided by coils 1' and 2' mounted on an uncoiling device which is not shown in the drawings. Furthermore on another coil 3' an intermediate thermoplastic layer 3 is provided.
  • Each metal strip 1, 2 is plasma coated by a plasma coating apparatus 4, which is described schematically beow.
  • a plasma coating apparatus 4 which is described schematically beow.
  • both metal strips 1, 2 are laminated to a composite strip 5 using a laminating apparatus 6 which is also shown schematically. It has been surprisingly found that plasma coating for coating the inner side of the metal layers 1, 2 with a plasma polymerized adhesion promoter layer is suitable for manufacturing a composite strip 5 in succession with a laminating process provided by the laminating apparatus 6.
  • the plasma coating step includes providing a process gas, generating a plasma at atmospheric pressure preferably between a first and a second electrode, injecting a precursor for providing the adhesion promoter layer into the plasma afterglow, moving the at least one metal substrate for example strip into plasma afterglow and depositing at least in part the plasma polymerized adhesion promoter layer on the surface of the inner side of the at least one metal strip.
  • a process gas generating a plasma at atmospheric pressure preferably between a first and a second electrode
  • injecting a precursor for providing the adhesion promoter layer into the plasma afterglow moving the at least one metal substrate for example strip into plasma afterglow and depositing at least in part the plasma polymerized adhesion promoter layer on the surface of the inner side of the at least one metal strip.
  • Fig. 2 shows a sectional view of a composite sheet 7 made from the composite strip 5 of Fig. 1 or alternatively made by stacking sheet material.
  • a composite sheet 7 consists of two metal layers 1, 2 for example made of steel which can be plated by zinc, zinc-magnesium, chromium-plated or plated on an aluminum-basis for corrosion resistance. Both metal layers 1, 2 comprise at the inner sides plasma polymerized adhesion promoter layers 1a, 2a made by depositing plasma polymerized organic carbon acid in particular acrylic acid or methacrylic acid onto the inner surface of the metal layers 1, 2.
  • Fig. 3 now shows the step of plasma coating of a metal layer 2.
  • the process gas containing N 2 and additional 3 vol.-% hydrogen flows between a first electrode 10 and a second electrode 9.
  • An aerosol 11 is injected into the plasma afterglow 13.
  • the aerosol is created by a support gas, presently containing N 2 and a precursor liquid, presently containing acrylic acid.
  • the precursor liquid may comprise allylamine, allylmethacrylate, (3-glycidoxypropyl)trimethoxysilane, (3-aminopropyl)triethoxysilane or preferred hydroxyethylacrylate and is directed together with the process gas 8 and the plasma onto the inner side of the metal layer 2.
  • the plasma 12 is generated between the first electrode 9 and the second electrode 10.
  • the plasma afterglow 13 extends to the surface of the inner side of a metal strip 1 or 2.
  • the aerosol 11 is directed into the plasma afterglow 13 and on the surface of the metal strip 1 or 2. This leads to a deposition of the plasma polymerized acrylic acid on the surface as adhesion promoter layer 2a.
  • the plasma 12 activates the inner surface of the metal strip 2 as well as the mixture of the aerosol comprising the precursor liquid directed to the surface of the metal layer 2.
  • a very thin indirect coating of a plasma polymerized adhesion promoter layer 2a is built on the surface of the metal strip 2.
  • the coated plasma polymerized adhesion promoter layer 2a has a thickness of 2 to 50 nm, preferably 5 nm to 30 nm. Due to the amount of hydrogen in the process gas 8 the peel test value rises additionally compared to peel test value achieved with a process gas without hydrogen.
  • Fig. 4 shows a second embodiment of a plasma coating step of a metal substrate 2'.
  • the plasma 12' is generated between the first electrode 10' and the second electrode 9'.
  • an aerosol 11' is injected into the plasma 12'. This leads to a direct coating of a plasma polymerized adhesion promoter layer on the surface of the metal substrate 2'.
  • a gaseous precursor can be injected alternatively.
  • Fig. 5 shows a third embodiment of a plasma coating step of a metal substrate 2".
  • the plasma 12" is generated between the second electrode 9" and the metal substrate 2" which acts as a first electrode 10". Indicated by an arrow an aerosol 11" or alternatively a gaseous precursor is injected into the plasma 12". A direct coating of a plasma polymerized adhesion promoter layer on the surface of the metal substrate 2" is applied.
  • the method for manufacturing composite sheets described here is able to provide composite sheets in an economical way with high peel test values independently of the coating of the metal substrates used for manufacturing the composite sheet.

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Plasma & Fusion (AREA)
  • Thermal Sciences (AREA)
  • Laminated Bodies (AREA)

Claims (12)

  1. Verfahren zur Herstellung einer Kompositwerkstoffplatte, wobei die Kompositwerkstoffplatte mindestens zwei äußere Metallschichten und mindestens eine zwischenliegende Polymerschicht umfasst, wobei die Polymerschicht ein thermoplastisches Polymer umfasst, wobei das Verfahren die Schritte umfasst:
    - Bereitstellen mindestens eines ersten und eines zweiten Metallsubstrats zum Bereitstellen der äußeren Metallschichten und mindestens einer zwischenliegenden Polymerschicht;
    - Beschichten mindestens eines der Metallsubstrate mit einer Haftvermittlerschicht durch Plasmabeschichten an der Innenseite des mindestens einen Metallsubstrats, wobei das Plasma bei Atmosphärendruck erzeugt wird und wobei die Innenseite des mindestens einen Metallsubstrats in Kontakt mit der mindestens einen zwischenliegenden Polymerschicht steht, wobei das Plasmabeschichten umfasst: das Bereitstellen eines Prozessgases, das Erzeugen eines Plasmas, das Injizieren eines Vorläufers zum Bereitstellen der Haftvermittlerschicht in das erzeugten Plasma oder Plasmanachglühen, Bewegen oder Positionieren des mindestens einen Metallsubstrats in das erzeugte Plasma oder Plasmanachglühen und das Absetzen mindestens teilweise einer plasmapolymerisierten Haftvermittlerschicht auf der Oberfläche der Innenfläche des mindestens einen Metallsubstrats;
    - Laminierens der mindestens einen Polymerzwischenschicht und der beiden äußeren Metallschichten, um ein Kompositwerkstoffmaterial herzustellen.
  2. Verfahren nach Anspruch 1,
    dadurch gekennzeichnet, dass
    der Vorläufer im flüssigen oder gasförmigen Zustand vorliegt.
  3. Verfahren nach Anspruch 1 oder 2,
    dadurch gekennzeichnet, dass
    ein Aerosol durch ein Trägergas und Verwenden einer Vorläuferflüssigkeit bereitgestellt wird umfassend organische Säure, insbesondere organische Carbonsäure, insbesondere eine Acrylsäure oder Methacrylsäure.
  4. Verfahren nach Anspruch 1 oder 2,
    dadurch gekennzeichnet, dass
    der flüssige oder gasförmige Vorläufer Allylamin, Allylmethacrylat, (3-Glycidoxypropyl)trimethoxysilan, (3-Aminopropyl)triethoxysilan oder bevorzugt Hydroxyethylacrylat umfasst.
  5. Verfahren nach einem von Anspruch 1 bis 4,
    dadurch gekennzeichnet, dass
    das Prozessgas N2, CO2, Ar und/oder He enthält.
  6. Verfahren nach Anspruch 5,
    dadurch gekennzeichnet, dass
    das Prozessgas ferner mindestens Wasserstoff als reaktives Gas umfasst, wobei das Prozessgas maximal 5 Vol.-% Wasserstoff umfasst.
  7. Verfahren nach einem von Anspruch 1 bis 6,
    dadurch gekennzeichnet, dass
    eine plasmapolymerisierte Haftvermittlerschicht in einer Dicke von 2 bis 50 nm auf der Innenseite mindestens einer Metallschicht abgesetzt wird.
  8. Verfahren nach einem von Anspruch 1 bis 7,
    dadurch gekennzeichnet, dass
    das Plasma bei Atmosphärendruck zwischen einer ersten Elektrode und einer zweiten Elektrode erzeugt wird.
  9. Verfahren nach einem von Anspruch 1 bis 8,
    dadurch gekennzeichnet, dass
    die Metallsubstrate unbeschichtete Stahlsubstrate oder Stahlsubstrate sind, die mit Zink, Zink-Magnesium plattiert, chromplattiert oder auf einer Aluminiumbasis oder Edelstahl, Aluminium und seine Legierungen oder Magnesium und seine Legierungen, Zink, Kupfer, Titan oder ihre Kombinationen plattiert sind.
  10. Verbundwerkstoffplatte bestehend aus mindestens zwei äußeren Metallschichten (1, 2) und mindestens einer thermoplastischen Zwischenpolymerschicht (3), wobei mindestens eine Innenseite einer äußeren Metallschicht eine plasmapolymerisierte Haftvermittlerschicht (1a, 2a) umfasst, die durch ein Verfahren nach Anspruch 1 bis 9 schichtförmig aufgebracht wird.
  11. Verbundwerkstoffplatte nach Anspruch 10,
    dadurch gekennzeichnet, dass
    die plasmapolymerisierte Haftvermittlerschicht (1a, 2a) eine Dicke von 2 nm bis 50 nm aufweist.
  12. Verbundwerkstoffplatte nach Anspruch 10 oder 11,
    dadurch gekennzeichnet, dass
    die äußeren Metallschichten aus einem unbeschichteten Stahlsubstrat oder einem Stahlsubstrat (1, 2) bestehen, das mit Zink, Zink-Magnesium plattiert, chromplattiert oder auf einer Aluminiumbasis plattiert ist oder aus Edelstahl, Aluminium und seinen Legierungen oder Magnesium und seinen Legierungen, Zink, Kupfer, Titan oder ihren Kombinationen hergestellt ist.
EP14151504.9A 2014-01-16 2014-01-16 Verbundfolie und Verfahren zur Herstellung Active EP2896502B1 (de)

Priority Applications (4)

Application Number Priority Date Filing Date Title
EP14151504.9A EP2896502B1 (de) 2014-01-16 2014-01-16 Verbundfolie und Verfahren zur Herstellung
PCT/EP2015/050779 WO2015107152A1 (en) 2014-01-16 2015-01-16 Composite sheet and method of manufacturing
CN201580004774.4A CN105939852B (zh) 2014-01-16 2015-01-16 复合片材及制造方法
US15/205,159 US20160318294A1 (en) 2014-01-16 2016-07-08 Composite sheet and method of manufacturing

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP14151504.9A EP2896502B1 (de) 2014-01-16 2014-01-16 Verbundfolie und Verfahren zur Herstellung

Publications (2)

Publication Number Publication Date
EP2896502A1 EP2896502A1 (de) 2015-07-22
EP2896502B1 true EP2896502B1 (de) 2017-03-08

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US (1) US20160318294A1 (de)
EP (1) EP2896502B1 (de)
CN (1) CN105939852B (de)
WO (1) WO2015107152A1 (de)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102015108237A1 (de) * 2015-05-26 2016-12-01 Thyssenkrupp Ag Herstellung von Verbundmaterial mittels Plasmabeschichtung
DE102015117201A1 (de) * 2015-10-08 2017-04-13 Bwg Bergwerk- Und Walzwerk-Maschinenbau Gmbh Verfahren und Anlage zum kontinuierlichen Herstellen von Verbundbändern oder -blechen
DE102016200667A1 (de) * 2016-01-20 2017-07-20 Thyssenkrupp Ag Verfahren und Vorrichtung zum Herstellen eines Werkstoffverbundes sowie dessen Verwendung
KR102008971B1 (ko) 2017-12-21 2019-08-08 주식회사 포스코 강판 및 작용기가 도입된 플라스틱층이 합지된 복합 소재 및 그 제조방법
CN110497659A (zh) * 2019-07-18 2019-11-26 尼尔金属(苏州)有限公司 一种复合材料及其制备方法及使用其的电子产品

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US3725169A (en) * 1971-06-11 1973-04-03 Anaconda Aluminum Co Bimetallic laminate and method of making same
JP2897055B2 (ja) * 1990-03-14 1999-05-31 株式会社ブリヂストン ゴム系複合材料の製造方法
AU2001247975A1 (en) * 2000-02-18 2001-08-27 University Of Cincinnati Plasma polymerized primers for metal pretreatment
DE60322347D1 (de) * 2002-02-05 2008-09-04 Dow Global Technologies Inc Chemische dampfphasenabscheidung auf einem substrat mittels eines korona-plasmas
GB0208261D0 (en) * 2002-04-10 2002-05-22 Dow Corning An atmospheric pressure plasma assembly
DE102004022677A1 (de) * 2004-05-07 2005-11-24 Bayer Materialscience Ag Vorrichtung und Verfahren zur Herstellung von Sandwich-Verbundelementen
DE102007046226A1 (de) * 2007-09-26 2009-04-09 Thyssenkrupp Steel Ag Verfahren zur Herstellung eines Leichtblechs
EP2589438B1 (de) 2011-11-07 2017-05-03 Vlaamse Instelling voor Technologisch Onderzoek (VITO) Plasmaoberflächenaktivierungsverfahren und daraus entstehendes objekt

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Also Published As

Publication number Publication date
EP2896502A1 (de) 2015-07-22
CN105939852A (zh) 2016-09-14
CN105939852B (zh) 2019-09-24
US20160318294A1 (en) 2016-11-03
WO2015107152A1 (en) 2015-07-23

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